GB 5009.256-2016 (GB5009.256-2016) & related versions
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National Standard of Food Safety -- Determination of Phosphates in Foods
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GB 5009.256-2016
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GB 5009.256-2016
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GB 5009.256-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Standard of Food Safety -
Determination of Phosphates in Foods
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 01, 2017
Issued by. National Health and Family Planning Commission of PRC
Table of Contents
1 Scope ... 3
2 Principle ... 3
3 Reagents and Materials ... 3
4 Apparatus ... 5
5 Analytical Procedures ... 5
6 Expression of Analytical Results ... 9
7 Precision ... 9
8 Others ... 9
Appendix A Conversion Factor of Polyphosphate Radical ... 11
Appendix B Five Different Phosphate Radical Standard Ion Chromatograms 12
National Standard of Food Safety -
Determination of Phosphates in Foods
1 Scope
This Standard specifies the determination of phosphates in foods.
This Standard is applicable to the determination of phosphate, pyrophosphate,
hexametaphosphate, trimetaphosphate, and tripolyphosphate in foods.
2 Principle
The specimen sampling shall adopt the corresponding method to extract and purify;
take the potassium hydroxide solution as the eluent; separated by anion exchange
column and detected by conductivity detector. Qualitative with retention time, and
quantified by external standard method.
3 Reagents and Materials
Unless otherwise stated, the reagents used in this method are all guarantee reagents;
while water is Level-I water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Sodium hydroxide (NaOH).
3.1.2 Potassium hydroxide (KOH).
3.1.3 Methanol (CH3OH) chromatographically pure.
3.2 Reagent preparation
3.2.1 Sodium hydroxide (10mmol/L). take 0.4g of sodium hydroxide; dissolve into
water; dilute and make constant volume of 1000mL.
3.2.2 Sodium hydroxide (50mmol/L). take 2.0g of sodium hydroxide; dissolve into
water; dilute and make constant volume of 1000mL.
3.3 Standard substance
5.2.1.3 Oil, fat, sauces. take 1g (accurate to 0.001g, the sampling quantity of the
specimen can be adjusted properly) of specimen; use 50mmol/L sodium hydroxide
solution to wash into 50mL colorimetric tube; mix evenly and make constant volume to
the scale; perform ultrasonic extraction at 80°C for 30min; shake once every 5min;
keep the stationary phase completely dispersed. After cooling to the room temperature,
the solution was filtered through filter paper; take filtrate at 4°C, centrifuge at 8000r/min
for 10min; take the supernatant for later-use.
5.2.1.4 Fish, meat and its products. take 2.5g (accurate to 0.001g, the sampling
quantity of the specimen can be adjusted properly) of specimen; use 50mmol/L sodium
hydroxide solution to wash into 100mL colorimetric tube; mix evenly and make
constant volume to the scale; perform ultrasonic extraction at 80°C for 30min; shake
once every 5min; keep the stationary phase completely dispersed. After cooling to the
room temperature, the solution was filtered through filter paper; take filtrate at 4°C,
centrifuge at 8000r/min for 10min; take the supernatant for later-use.
5.2.2 Sample purification
Take approximately 15mL of supernatant after treatment in 5.2.1; pass through a
0.45µm aqueous membrane needle filter; OnGuard II RP; discharge the first 3mL (if
the chloride ion is greater than 100mg/L, then successively pass through needle filter,
OnGuard II RP, Ag column and Na column, discharge the first 7mL); collect the back
eluent to be tested. Appropriately dilute the to-be-tested solution as per the sample
content before measurement.
The solid phase extraction column needs to be activated before use; e.g. when using
OnGuard II RP column (1.0mL), OnGuard II Ag column (1.0mL) and OnGuard II Na
column (1.0mL), their activation processes are as follows. before use, the OnGuard II
RP column (1.0mL) shall successively be passed through by 10mL of methanol and
15mL of water; stand and activate for 30min. For OnGuard II Ag column (1.0mL) and
OnGuard II Na column (1.0mL), they shall be passed through by 10mL of water; stand
and activate for 30min.
5.3 Reference chromatographic conditions
5.3.1 Chromatographic column. the selection of hydroxide can be compatible with
the gradient elution high volume anion exchange column, such as Dionex lonpac AS11-
HC 4mm×250mm (with Ionpac AG11-HC type guard column 4mm×50mm), or ion
chromatographic column with equivalent functions.
5.3.2 Eluent. potassium hydroxide solution; the gradient elution time and potassium
hydroxide concentration can refer to Table 2, flow rate of 1.0mL/min.
for trimetaphosphate radical, 4.8mg/kg for hexametaphosphate radical, respectively;
while their quantitative limits are as follows. 5.0mg/kg for phosphate radical, 5.0mg/kg
for pyrophosphate radical, 5.0mg/kg for tripolyphosphate radical, 5.0mg/kg for
trimetaphosphate radical, 15mg/kg for hexametaphosphate radical, respectively.
b) Vegetables, fruits, jellies, chocolate and candies, miscellaneous grains, wheat flour
and products, milk powder, dairy beverages or beverages. take 2.5g of sample; make
constant volume of 50mL; dilute 5 times before test; the detection limits for various
polyphosphate radicals are tested as follows. 3.0mg/kg for phosphate radical,
2.8mg/kg for pyrophosphate radical, 3.0mg/kg for tripolyphosphate radical, 3.2mg/kg
for trimetaphosphate radical, 9.6mg/kg for hexametaphosphate radical, respectively;
while their quantitative limits are as follows. 10mg/kg for phosphate radical, 10mg/kg
for pyrophosphate radical, 10mg/kg for tripolyphosphate radical, 10mg/kg for
trimetaphosphate radical, 30mg/kg for hexametaphosphate radical, respectively.
c) Oils, fats, sauces. take 1.0g of sample; make constant volume of 50mL; take 2.5g
of fish and meat samples; make constant volume of 100mL; dilute 2.5 times before
test; the detection limits for various polyphosphate radicals are tested as follows.
6.0mg/kg for phosphate radical, 5.6mg/kg for pyrophosphate radical, 6.0mg/kg for
tripolyphosphate radical, 6.4mg/kg for trimetaphosphate radical, 19.2mg/kg for
hexametaphosphate radical, respectively; while their quantitative limits are as follows.
20mg/kg for phosphate radical, 20mg/kg for pyrophosphate radical, 20mg/kg for
tripolyphosphate radical, 20mg/kg for trimetaphosphate radical, 60mg/kg for
hexametaphosphate radical, respectively.
......
| Standard ID | GB 5009.256-2016 (GB5009.256-2016) | | Description (Translated English) | National Standard of Food Safety -- Determination of Phosphates in Foods | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 8,856 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-03-01 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 |
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